37 Egypt. J. Chem. 59, No.4, pp.623 –636 (2016)

Utilization of GBFS in The Preparation of Low

Cost Cement

H. El-Didamony, M. Heikal*, H. Moselhy

**, M.A. Ali

***

Faculty of Science, Zagazig University, Zagazig , *Chemistry

Department, Faculty of Science, Benha University, Benha, **

Higher Institute of Engineering, El-Sohrouk Academy, El-

Sohrouk and ***

Faculty of Pharmacy, Badr University in Cairo,

Badr City, Egypt.

ROUNDED blast furnace slag GBFS is one of common

supplementary cementitious materials in Portland cement

concrete, and is capable of improving the performance of concrete and

reducing the costs. There are strong environmental and energy reasons

for developing a wide range of pozzolanic cements. The aim of this

work is to study the effect of substitution of cement with GBFS by the

determination of water of consistency, initial and final setting times,

combined water and free lime contents, bulk density, total porosity and

compressive strength. The results show that the substitution of GBFS

decreases the water of consistency, initial and final setting times, 50 %

GBFS increases compressive strength as well as total porosity,

whereas the free lime and combined water decrease with the

granulated slag content. The hydration products of some GBFS cement

pastes were identified by the aid of XRD, DTA and IR techniques.

Keywords: Granulated slag GBFS, Hydration, Compressive strength,

Blk density and Total porosity.

Ground granulated slag is one of the most important supplementary cementitious

materials in cement paste, and has been widely used in modern concrete because

of its several well-known advantages. For instance, GBFS is capable of

improving the resistance of concrete to chloride ingress, it can also reduce the

total heat generation and peak temperature reached during the early stage of mass

concrete structure, which lessens the risk of early-age thermal cracking(1-3)

.

Power plants using coal or rice husks as fuel and metallurgical furnaces

producing pig iron, steel, copper, nickel, lead, silicon and ferrosilicon alloys are

major sources of by-products. These by-products must be disposed off in a

suitable way. Disposal by dumping represents a resource of waste and causes

environmental problems. Exploiting the pozzolanic and the cementitious

properties of these materials by incorporating as components of Portland cement

concrete, represents high value of applications.

Blast-furnace slag has no cementitious value; but when it is quenched in

excess water and then ground, it acquires cementitious value. The process of

quenching is called “granulation” and the product is “granulated blast-furnace

slag” (GBFS).

G

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

624

Granulated blast-furnace slag (GBFS) is a nonmetallic, rapidly chilled

alumino-silicate material that separated from molten iron in the blast-furnace.

Granulated slag issues from the blast-furnace as a molten stream at temperatures

1400 –500 °C from reaction of silica and alumina as acidic oxides with calcium

and magnesium as basic oxides to form slag in the presence of other oxides of

iron, sodium, potassium and sulfides as minor components(4)

. Cooling is most

often effected by spraying droplets of the molten slag with high-pressure jets of

water. This gives a wet, sandy material which when dried and ground is called

granulated blast-furnace slag GBFS and often contains over 95% of glass.

The Tunisian blast-furnace slag has been characterized by several

physicochemical methods to evaluate its hydraulic reactivity(5)

. It has been noted

that nearly all the GBFS is glassy, so its use as a replacement of cement is

possible. This result has been confirmed by different physical tests applied to

pozzolanic cements as specific surface area, normal consistency, setting time,

stability to expansion and the minislump.

The replacement of a part of clinker by GBFS has led to the following results:

an acceptable extension of the setting time, an improvement of the

rheological behavior, and a very good stability to expansion,

an improvement of the compressive strength at 28 days, but with a slight

decrease at 7 days.

GBFS is the most useful latent hydraulic material, because the amount

produced is very large and its properties are very stable compared with other

industrial by-products(6)

.

Bágel(7)

studied the workability and incorporating granulated blast furnace

slag and silica fume composite cement mortars. The compressive strength and

mercury intrusion were tested for plain Portland cement mortar and/or slag-

cement mortar. The results showed that with high portions of GBFS and SF in the

binding system, the mortars reached relatively satisfactory level of compressive

strength and contributed to the significantly denser pore structure.

The aim of the present work is to establish the optimum composition of slag

cement made from granulated blast-furnace slag and OPC. Different blends were

prepared from these materials and the physico-mechanical properties were

studied. The water of consistency , initial and final setting times, combined water,

free lime as well as bulk density, total porosity and compressive strength are

determined.

Experimental

The materials used in this investigation were Imported granulated blast-

furnace slag supplied by (Kokan Mining Co. LTD, Japan) and ordinary Portland

cement (OPC) from Suez Cement Company. The chemical analysis of these raw

Utilization of GBFS in The Preparation of Low…

Egypt. J. Chem. 59, No.4 (2016)

625

materials are shown in Table 1. The X-ray diffraction of granulated slag is seen

in Fig. 1. Generally, the granulated slag is nearly completely vitreous with an

amorphous hump characteristic of the glass at 28 2. This corresponds to a 2

value of 30.70 2 consistent with those of the amorphous phase being constituted

of network-forming oxides SiO2 and Al2O3.

Different mixes were made by substitution of 70, 60, 50, 40 wt. % OPC by

GBFS. The mixes were denoted as A1, A2, A3, and A4 as shown in Table 2.

TABLE 1. Chemical composition of starting materials, (wt%).

Oxides

Materials

SiO

2

Al 2

O3

Fe 2

O3

Ca

O

Mg

O

Na

2O

K2O

Ba

O

SO

3

S--

L.O

.I

WCS 37.48 12.86 0.40 37.70 2.45 1.84 0.93 5.31 0.01 0.75 ـــــ

OPC 20.51 5.07 4.39 62.21 2.00 0.23 0.29 2.40 ـــــ 2.25 ــــــ

Fig. 1. XRD pattern of imported granulated slag.

TABLE 2. Mix composition of the prepared cements, (wt %).

Mix No. OPC GBFS

A1 30 70

A2 40 60

A3 50 50

A4 60 40

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

626

Each dry mix was homogenized on a roller in a porcelain ball mill with four

balls for 1 hr to assure complete homogeneity. The water demand for standard

consistency and setting time were measured (ASTM Designation: C191, 2008)(8)

.

The pastes were mixed with the water of consistency and moulded into stainless

steel (2×2×2 cm) cubic moulds, cured in a 100 % R.H at 23 ± 1°C for the first

24hr, then demolded and cured under water until the desired curing time such as

3, 7, 28, 90 and 180 days was reached. The compressive strength was carried out

on four samples. The procedure described by ASTM Specifications (ASTM

Designation: 150, 2007)(9)

. Four cubes were used for the determination of

compressive strength of the hardened pastes at any given condition. The

compressive strength measurements were done on a compressive strength

machine of SEIDNER, Riedlinger, Germany, having maximum capacity of 600

KN force. The broken specimens were immersed in water to avoid loss of water

filling the pores, and then collected for further testing.

After the predetermined curing time, the hydration of the paste was stopped by

the removal of free water. About 10 grams of the crushed paste, after compressive

strength testing, were ground and dried at 70°C for about 3 hr to remove the free

water. The resulted dried samples were then stored in desiccators for other physico-

chemical measurements. The kinetics of hydration was followed by the

determination of the free lime according to BS EN 196-2:2013(10)

. The portlandite

content of cement paste can be thermally determined. 0.5 g of the hardened cement

was placed in a porcelain crucible and introduced into a cold muffle furnace. The

temperature was increased up to 390 then to 550°C at heating rate of 3 C/min. The

loss of weight occurring between 390 and 550 °C with soaking time of 15 min is

equal to the weight of water of calcium hydroxide. Therefore, the free lime can be

calculated (11)

. The combined water content was determined by the ignition loss of

the dried paste at 850 ºC for 20 minutes based on ignited weight basis minus the

loss of the anhydrous blend (12)

. The compressive strength was determined up to

180 days. The bulk density and total porosity, ξ, was calculated by weighing the

saturated sample as (W1), then suspended in water (W2) and finally dried weight

after drying at 105oC for 24 hr,

(W3) bulk density = g/cm3 , The total porosity = * 100

Results and Discussion

Water of consistency and setting time

The results of water of consistency and setting times of slag cement pastes are

shown in Fig. 2. The substitution of GBFS by Imported OPC increases the water of

consistency of cement pastes. This may be due to the lower hydraulic properties of

Imported GBFS in comparison with OPC. The OPC is hydraulic cement which

needs more water of mixing than GBFS cement pastes therefore the water of

W1 ــــــــــــــــــــ

w1-w2

W1-w3* ــــــــــــــــــ

w1-w2

Utilization of GBFS in The Preparation of Low…

Egypt. J. Chem. 59, No.4 (2016)

627

30 40 50 60

26.4

26.6

26.8

27.0

27.2

27.4

W/C %

Initial

Final

Wat

er o

f con

sist

ency

, %

Initi

al a

nd fi

nal S

ettin

g tim

e (m

in.)

OPC content, wt%

200

220

240

260

280

300

320

340

360

380

400

1 10 100

6

7

8

9

10

11

12

13

14

15

Comb

ined w

ater %

Curing time, days

A1

A2

A3

A4

consistency increases with OPC content. The elongation of initial and final setting

times with the decrease of the GBFS content is mainly attributed to the low

hydraulic properties of GBFS. This elongates the initial and final setting times of

cement paste. The decrease of initial and final setting times of cement pastes at

50% OPC is mainly attributed to the increase of OPC on the expense of GBFS.

Fig. 2. Water of consistency and setting time of slag cement pastes.

Combined water content The combined water contents of hydrated GBFS cement pastes are graphically represented as a function of curing time in Fig. 3. The combined water contents increase gradually with curing time up to 180 days for all cement pastes. This is due to the continuous hydration and accumulation of hydration products as C-S-H and AFt & AFm. GBFS reacts very slowly with water but without setting

(13) . The results also show that the combined water contents of

GBFS cement pastes decrease with slag content. This is mainly due to the slow hydration reaction of slag grains at early ages. As the amount of OPC increases, the combined water content increases. This may be attributed to the formation of large amounts of C-S-H with OPC content.

Fig. 3. Combined water contents of granulated slag cement pastes up to 180 days.

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

628

1 10 100

0.5

1.0

1.5

2.0

2.5

3.0

Free

lim

e con

tent

, (%

)

Curing time, days

A1

A2

A3

A4

15 20 25 30 35 40 45 50 55 60

CCCSH

C3S

C2S

A3 180 days

Inten

sity

2- Theta - Scale

A3 3 days

CH

Free lime content The free lime contents of hydrated slag cement pastes are graphically

represented as a function of curing time in Fig. 4. The results show that the free lime content increases with the increase of the amount of C3S and β-C2S, which are the main source of free lime during the hydration of cement pastes. On the other side, the rate of consumption of the free lime of slag cement pastes increases with the amount of GBFS in the GBFS cement blends. This is associated with the hydration reaction of the GBFS and the free lime released from clinker hydration in addition to the decrease of clinker portion in the cement blends. Pozzolanic cement pastes with high content of GBFS show slow rate of liberation due to its lower hydraulic properties and its consumption of free lime.

Fig. 4. Free lime contents of slag cement pastes up to 180 days.

Figure 5 shows the XRD diffractograms of the hardened GBFS cement pastes

made of mix A3 (50% OPC + 50% GBFS) cured at 3 and 180 days. It is found that the intensity of characteristics lines for calcium hydroxide (CH) (4.92 Å, 2.62 Å, 1.92 Å and 1.79 Å), decreases with curing time. This is due to the continuous consumption of Ca(OH)2 with GBFS in pozzolanic reaction. Also, the peaks of unhydrated phases of β-C2S and C3S decrease with curing time due to the continuous hydration of β-C2S and C3S. The CaCO3 (CC) is also detected and overlapped by CSH at 3.03 Å.

Fig. 5. X-ray diffraction patterns of hardened cement pastes with (50% OPC + 50%

GBFS) immersed in tap water up to 180 days.

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Egypt. J. Chem. 59, No.4 (2016)

629

4000 3600 3200 2800 2400 2000 1600 1200 800 400

70

80

90

100

110

120

130

Tran

smitt

ance

, %

Wavenumbers, cm-1

2339

2364

2927 16

33

877

1433

985

518

3440

(2)

(1)

(1) A3 3 days

(2) A3 180 days

Figure 6 shows the FTIR spectra of hydrated GBFS cement pastes as a

function of curing time. It is clear that the intensity of the band at 3640 cm−1

related to OH– group increases with curing time up to 180 days. This is due to the

increase of liberated lime from OPC cement phases.

The broad band near 3436 cm−1

due to stretching band ν1 + ν2 of H2O

increases with curing time. In addition, the band at 1643 cm−1

is related to the

bending ν2 of H2O and indicates the formation of CSH (14)

. The band at 985 cm−1

due to that CSH increases from 3 days up to 180 days. The absorption band at

1433 cm-1

is due to the presence of ν3 CO3-2

as well as 877 cm-1

(ν2) that formed

from carbonation of Ca(OH)2.

Fig. 6. FTIR spectroscopy of A3 (50% OPC + 50% GBFS) cured at 3 and 180 days

under tap water.

Bulk density and total porosity

The bulk density and total porosity of GBFS cement pastes cured up to 180

days are shown in Fig. 7 and 8, respectively. The bulk density of the hardened

cement pastes increases and the total porosity decreases with curing time due to

the filling of some pores by hydration products. The bulk density decreases and

the total porosity increases with slag content. This is mainly due to the decrease

of GBFS density in addition to the low rate of hydration which forms hydration

products with high bulk densities such as C-S-H gel. A4 40/60 GBFS : OPC

gives the higher bulk density, i.e. increases with OPC content. The C-S-H formed

from slag cement paste gives lower bulk density than that of Portland cement.

The decrease of total porosity at later ages is mainly due to the higher pozzolanic

reaction of GBFS with CH at later ages (13)

.

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

630

Fig. 7. The bulk density of imported GBFS rich cement pastes with curing time.

Fig. 8. The total porosity of imported GBFS rich cement pastes with curing time.

Compressive strength

The results of compressive strength of GBFS cement pastes cured up to 180

days are graphically plotted in Fig. 9. It is clear that the compressive strength

increases with curing time for all GBFS cement pastes. As the hydration

proceeds, more hydration products and cementing materials are formed. This

leads to increase the compressive strength of hardened cement pastes. The

hydration products possess a large specific volume than unhydrated cement

compounds. Therefore, the accumulation of the hydrated products will fill a part

of the originally filled spaces which leads to decrease the total porosity and

increase the compressive strength of the cement paste. The compressive strength

decreases with GBFS content. This is due to the lower β- C2S and C3S content in

slag cement blends, which is responsible for the formation of CSH and CH upon

hydration that accelerates also the hydration of GBFS. Therefore, the

compressive strength decreases at early ages of hydration but at later ages of

hydration (180 days), the GBFS cement pastes contribute strongly to the

developed compressive strength. These results of compressive strength are

compatible and in agreement with the total porosity, bulk density, and combined

Utilization of GBFS in The Preparation of Low…

Egypt. J. Chem. 59, No.4 (2016)

631

water of GBFS cement pastes. Pozzolanic cement admixed with 40 and 50 wt%

GBFS shows higher strength values at later ages due to the increase of pozzolanic

activity of GBFS at later ages.

Thermo-gravimetric analysis

The hydration products of the GBFS rich cement pastes can be investigated

from the DTA of the hydrated cement pastes.

Fig. 9. The Compressive strength of imported slag rich cement pastes up to 180 days.

Figure 10 illustrates the DTA thermograms of Mix A3 with 50 wt% GBFS at

3 and 180 days. The thermograms show endothermic peaks at 100 °C, 150 °C ,

200 °C, 215 °C, 475 °C, 700-900°C in addition to an exothermic peak at 955 °C.

The first endothermic peak is characteristic to the decomposition of CSH as well

as tobermorite like phase(15)

. The second peak at 150–200°C is related to

C2ASH8. Whereas the endotherms at 215 °C and ≈ 417 °C are represented to the

decomposition of calcium aluminate hydrate C4AH13 and hydrogarnet series (16).

The endothermic peak at 427C is due to the decomposition of Ca(OH)2,

endothermic peaks at 555–674 C are due to decomposition of calcium carbonate

and hydrated aluminates as well as the final stage of C–S–H(13)

. Also, the

endothermic peaks from 550–960 are related to the decomposition of different

forms of carbonates. The exothermic peak at 955 o

C is mainly characteristic to

wollastonite which is developed during the process of crystallization of

monocalcium silicate (CS). This characteristic exothermic peak is related to the

hydrated calcium silicate formed from the hydration of pozzolanic materials such

as GBFS activated with Ca(OH)2.

Figure 10 illustrates the presence of C-S-H, CAH, C2ASH8 in addition to

hydrogarnet series at low temperature range before 450 o

C as hydration products

of mix A3. The thermograms show also the peak of Ca(OH)2 at 456 oC and the

endotherm in the range 700 – 900 oC due to decomposition of CaCO3 in addition

to the exotherm at 955 oC. It is clear that the amount of hydration products

increases with curing time due to continuous hydration of GBFS with the

liberated Ca(OH)2. The presence of a detectable endothermic peaks from the

dissociation of small amounts of Ca(OH)2 in the hydrated cement pastes is

mainly due to the great magnification of the thermograms because the chemical

analysis gives low values of free Ca(OH)2 .

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

632

Fig. 10. The DTA thermograms of hydrated

and 180 days.

Fig. 11. The DTA thermogram of hydrated

days.

The effect of the amount of GBFS in c

DTA thermograms of the hydrated ceme

days in Fig.13. It is clear that all hydrated

products in addition to free Ca(OH)2, CaC

wollastonite. It is also seen that the endo

range due to the decomposition of hydra

content or decrease of GBFS content. T

GBFS gives higher values of hydration pro

hydrated mixes. As the slag content in

hydration products as seen from the endot

due to the higher degree of hydration of c

other side, the hydration products of

GBFS rich cement paste of Mix A3 at 3

GBFS cement paste of A1 and A3 at 180

ement paste can be also seen from the

nt pastes of mixes A1 and A3 at 180

cement pastes show the same hydration

O3 and the exotherm of the formation

thermic peaks at the low temperature

tion products increase with the OPC

his means that mix A3 with 50 wt%

ducts as seen from the peak area of the

creases on the expense of OPC the

hermic peaks decrease. This is mainly

linker in comparison to GBFS. On the

pozzolanic cement pastes give low

Utilization of GBFS in The Preparation of Low…

Egypt. J. Chem. 59, No.4 (2016)

633

combined water content. On the other side, the peak area of Ca(OH)2 decreases

with the GBFS content. The liberated Ca(OH)2 is proportional to the amount of

Portland cement clinker or β-C2S and C3S which are the main source of free lime.

Therefore, the peak area of mix A3 > A1. The exotherm at 955 °C increases with

the amount of GPFS has the opposite direction of free Ca(OH)2. The exothermic

peak is proportional to the amount of C-S-H gel which is formed from the

hydration of GBFS with lime liberated from the hydration of Portland cement

clinker.

Figure 12 shows the TG thermograms of GBFS rich cement pastes with 50

wt% GBFS cured at 3 and 180 days. The combined water contents of cement

pastes are 9.074 and 13.923 wt% after 3 and 180 days. These losses occurred at

nearly 580 °C before the dehydroxylation of Ca(OH)2 and the calcinations of

CaCO3. It is clear that the combined water contents increase with curing time.

The cement pastes cured for 3 and 180 days , respectively give weight loss 11.54

and 18.42 wt% after firing at about 990 °C. The combined water as determined

by chemical method includes the loss of Ca(OH)2 as well as CaCO3. The cement

pastes Mix A1 and A3 are seen in Fig. 13. It is clear that the cement is more

hydraulic than GBFS and these values are in according with the determined

values of combined water.

Fig. 12. The TGA thermograms of hydrated GBFS rich cement paste of Mix A3 at 3

and 180 days.

Fig. 13. The TGA thermogram of hydrated GBFS cement paste of A1 and A3 at 180

days.

H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

634

Conclusions

From the above findings it can be concluded that:

1. GBFS decreases the water of consistency and shortens the setting time,

2. GBFS decreases the combined water content at well as the compressive

strength at early ages but at later ages 50 % GBFS has the higher

compressive strength.

3. The bulk density and the free lime decrease but the total porosity increases

with GBFS content.

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H. El-Didamony et al.

Egypt. J. Chem. 59, No.4 (2016)

636

إستخذام خبث الحذيذ المبرد مائيا في تحضير أسمنت رخيص التكلفة

محمذ أحمذ هيكلحمذى الذيذاموني أحمذ ، *

، حسام مصيلحي **

و محمذ أحمذ

علي***

، خبعخ اشلبسيك –ويخ اع –لس اىييبء * –ويخ اع –لس اىييبء

، خبعخ ثب**

أوبدييخ اشزق –اعذ اعب ذسخ –لس اذسخ اىييبئيخ

***

ظز . – خبعخ ثذر ثبمبزح –ويخ اظيذخ

عزجز خجث أفزا احذيذ برح ثب ع طبعخ احذيذ. يز إزبج ويبد ضخخ ي

و عب. ذه فإ إسزخذا ذ افبيبد ف ازبج اخزسبخ يفز ابي يحبفظ

ع اجيئخ. خذ أ خجث أفزا احذيذ يحس خاص األسذ ايىبيىيخ

ة اخبطخ ثزفيز اطبلخ احبفظخ ع افيشيموييبئيخ. بن اعذيذ األسجب

اجيئخ از أدد إ رطيز اعذيذ األسزبد اجساليخ. اذف ذا اجحث

حجت . ر إخزاء إخزجبراد دراسخ رأثيز إسزجذاي األسذ ثخجث أفزا احذيذ ا

ليبص سجخ بء اخط س اشه اإلثزذائ ابئ رعيي ابء ازحذ وييبئيب

ويخ اديز احز اىثبفخ اىيخ اسبيخ لح رح اضغط. خالي ذ

-: اذراسخ أى ازط إ ثعض ازبئح خشب فيب ي

اشه اإلثزذائ ابئ وذه لح رح اضغط خذ أ ويخ بء اخط س

رشداد ع سيبدح اسزجذاي خجث أفزا احذيذ احجت ثبالسذ اجررالذ. ثيب

ويخ ابء ازحذ وييبئيب ويخ اديز احز رزبلض ع ويخ خجث أفزا احذيذ

احجت.